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jiakangle2

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l-Brom[2.2]paracyclophan (3): In einem 2-I-Dreihalskolben rnit Tropftrichter, KPG-Riih-
rer  und  RiickfluDkiihler rnit  Gasableitungsrohr  werden  10.0 g (48 mmol) 1 in  1200 ml  absolutem  Tetrachlorkohlenstofl  in  der  Siedehitze gelost. Unter  dauernder  Bestrahlung  rniteiner  2000-Watt-Halogen-Tageslichtlampe werden  innerhalb  1 h  3.0 ml  (9.4  g,  59 mmol) Brom  zugetropft.  Nach  vollstiindiger Zugabe  wird  die  Losung  weitere  20 min  bestrahlt, abgekiihlt  und  auf  ca.  100 ml  eingeengt, wobei das schwer losliche Edukt  1 (3 g) ausfiillt. Dieses wird abgesaugt und das Filtrat zur Trockne eingeengt. Das so erhaltene Rohprodukt wird  saulenchromatographisch  (CC14) gereinigt:  7.2 g  (53%) 3,  farblose  Nadeln,  Schmp. 122¡ãC).
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°®ÓëÓêÏÂ(½ð±Ò+1): 2011-11-01 08:40:23
jiakangle2(½ð±Ò+30, ·­ÒëEPI+1): 2011-11-01 09:58:55
1-äå[2,2] ¶Ô¶þ¼×±½»·¶þÌå(3)£ºÔÚ´øÓеÎҺ©¶·£¬KGP½Á°èÆ÷ºÍÁ¬ÓÐÆøÌåµ¼¹ÜµÄ»ØÁ÷ÀäÄý¹ÜµÄ2ÉýÈý¿ÚÉÕÆ¿ÖмÓÈë10.0gµÄ1(48mmol)ºÍ1200mLÎÞË®ËÄÂÈ»¯Ì¼£¬¼ÓÈÈÖÁ·ÐÌÚ£¬Èܽ⡣ÔÚ2000WµÄ±¹âµÆ³ÖÐøÕÕÉäÏ£¬ÓÚ1СʱÄڵμÓÍê3.0mLäå(9.4g.£¬59mmol)ºó£¬¼ÌÐø¹âÕÕ20min£¬ÀäÈ´£¬Å¨ËõÖÁÔ¼100mL£¬´ËʱÄÑÈܵķ´Ó¦Îï1£¨3g£©Îö³ö¡£³éÂË£¬ÂËҺŨËõÖÁ¸É£¬ËùµÃµÄ´ÖÆ·¾­Öù²ãÎö´¿»¯£¨ËÄÂÈ»¯Ì¼£©µÃ£º7.2g(53%)3£¬ÎÞÉ«Õë×´¾§Ì壬ÈÛµã121¶È(ÎÄÏ×3a)122¶È)¡£
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cartman

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°®ÓëÓêÏÂ(½ð±Ò+1): 2011-10-31 20:02:56
jiakangle2(½ð±Ò+20): 2011-11-01 09:59:01
ÍùÁ¬½ÓÓеÎҺ©¶·£¬KGP½Á°èÆ÷ºÍ»ØÁ÷ÀäÄý¹Ü£¨Á¬ÓÐÅÅÆø¹Ü£©µÄ2ÉýÈý¿ÚÉÕÆ¿Àï¼ÓÈë10.1gµÄ1ºÍ1200mlÎÞË®ËÄÂÈ»¯Ì¼£¬»ØÁ÷ÈÜÇå¡£ÔÚ2000wµÄ±¹âµÆÕÕÉäÏ£¬ÓÚ1СʱµÎÈë3mlä壬¼ÓÍêºó£¬¼ÌÐø¹âÕÕ20min£¬ÀäÈ´£¬Å¨ËõÖÁÔ¼100ml£¬´ËʱÄÑÈܵķ´Ó¦Îï1£¨3g£©Îö³ö¡£³éÂË£¬ÂËҺŨËõÖÁ¸É¡£µÃµ½µÄ´ÖÆ·¹ýÖù´¿»¯£¨ËÄÂÈ»¯Ì¼£©£º7.2g3£¬ÎÞÉ«¾§Ì壬ÈÛµã121¶È¡£
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